# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_coden_ASTM ? _journal_coeditor_code ? _journal_coeditor_name ? _journal_coeditor_notes ; ? ; #============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_data_validation_number ? _journal_date_accepted ? _journal_date_from_coeditor ? _journal_date_printers_final ? _journal_date_printers_first ? _journal_date_proofs_in ? _journal_date_proofs_out ? _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_paper_category ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_volume ? _journal_year ? loop_ _publ_author_name _publ_author_address R.M.P.Colodrero ;Dpto Quimica Inorganica, Cristalografia y Mineralogia Facultad de Ciencias, Campus de Teatinos s/n 29071 M\'alaga Spain ; P.Olivera-Pastor ;Dpto Quimica Inorganica, Cristalografia y Mineralogia Facultad de Ciencias, Campus de Teatinos s/n 29071 Malaga Spain ; E.R.Losilla ;Dpto Quimica Inorganica, Cristalografia y Mineralogia Facultad de Ciencias, Campus de Teatinos s/n 29071 Malaga Spain ; M.A.G.Aranda ;Dpto Quimica Inorganica, Cristalografia y Mineralogia Facultad de Ciencias, Campus de Teatinos s/n 29071 Malaga Spain ; ; L.Leon-Reina ; ;Servicios Centrales de Apoyo a la Investigacion Universidad de Malaga, Campus Teatinos s/n, 29071 Malaga Spain ; M.Papadaki ;Crystal Engineering, Growth and Design Laboratory Department of Chemistry University of Crete, Voutes Campus Crete, GR-71003 Greece ; A.C.McKinlay ;School of Chemistry, University of St Andrews, Purdie Building St Andrews, KY16 9ST, UK ; R.E.Morris ;School of Chemistry, University of St Andrews, Purdie Building St Andrews, KY16 9ST, UK ; K.D.Demadis ;Crystal Engineering, Growth and Design Laboratory Department of Chemistry University of Crete, Voutes Campus Crete, GR-71003 Greece ; A.Cabeza ;Dpto Quimica Inorganica, Cristalografia y Mineralogia Facultad de Ciencias, Campus de Teatinos s/n 29071 Malaga Spain ; loop_ _publ_author_footnote ; ? ; _publ_contact_author_address # Address of author for correspondence ;Dpto. Quimica Inorganica, Cristalografia y Mineralogia Universidad de Malaga Facultad de Ciencias, Campus de Teatinos s/n 29071-Malaga (Spain) ; _publ_contact_author_email aurelio@uma.es _publ_contact_author_fax '+34 952131870' _publ_contact_author_phone '+34 952131877' #============================================================================= # this information describes the project, paper etc. for the CIF # # Acta Cryst. Section C papers and editorial correspondence is generated # # from the information in this section # # # # (from) CIF submission form for Rietveld refinements (Acta Cryst. C) # # Version 14 December 1998 # #============================================================================= # 1. SUBMISSION DETAILS _publ_contact_author_name 'Aurelio Cabeza Diaz' # Name of author for correspondence _publ_contact_letter ; ? ; _publ_requested_category ? # Acta C: one of CI/CM/CO/FI/FM/FO _publ_requested_coeditor_name ? #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; ? ; data_LAH5DTMP_ANH_publ _database_code_depnum_ccdc_archive 'CCDC 810315' #TrackingRef 'web_deposit_cif_file_0_RosarioMPerezColodrero_1323857331.LAHDTMP_ANH.cif' _ccdc_journal_manuscript_code DT-ART-10-2011-01199 _pd_block_id 2011-12-08T19:32|LAHDTMP_ANH_REV2|LaHDTMP_ID31|X'Pert_Pro _audit_creation_method 'from EXP file using GSAS2CIF' _audit_creation_date 2011-12-08T19:32 _audit_author_name LaH5DTMP_ANH _audit_update_record ; 2011-12-08T19:32 Initial CIF as created by GSAS2CIF ; _publ_section_title_footnote ; ? ; #============================================================================== # 4. TEXT _publ_section_synopsis ; ? ; _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_exptl_prep # Details of the preparation of the sample(s) # should be given here. ; ? ; _publ_section_exptl_refinement ; ? ; _publ_section_references ; ? ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; #============================================================================= # 5. OVERALL REFINEMENT & COMPUTING DETAILS _refine_special_details ; ? ; _pd_proc_ls_special_details ; ? ; # The following items are used to identify the programs used. _computing_molecular_graphics ? _computing_publication_material ? _refine_ls_weighting_scheme ? _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_number_constraints ? _refine_ls_restrained_S_all ? _refine_ls_restrained_S_obs ? #============================================================================== # 6. SAMPLE PREPARATION DATA # (In the unusual case where multiple samples are used in a single # Rietveld study, this information should be moved into the phase # blocks) # The following three fields describe the preparation of the material. # The cooling rate is in K/min. The pressure at which the sample was # prepared is in kPa. The temperature of preparation is in K. _pd_prep_cool_rate ? _pd_prep_pressure ? _pd_prep_temperature ? _pd_char_colour ? # use ICDD colour descriptions _refine_ls_shift/su_max 0.03 _refine_ls_shift/su_mean 0.01 _computing_structure_refinement GSAS _refine_ls_number_parameters 105 _refine_ls_goodness_of_fit_all 2.75 _refine_ls_number_restraints 65 _refine_ls_matrix_type full #============================================================================== # 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA _pd_char_particle_morphology ? _chemical_name_systematic ; ? ; _chemical_name_common 'LaH5DTMP ANH' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_melting_point ? _chemical_compound_source ? # for minerals and # natural products _symmetry_space_group_name_Hall ? _exptl_crystal_F_000 ? _exptl_crystal_density_diffrn ? _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _cell_measurement_temperature 473 _cell_special_details ; ? ; _geom_special_details ? # The following item identifies the program(s) used (if appropriate). _computing_structure_solution ? #============================================================================== # 8. Phase information from GSAS _pd_phase_name LaH5DTMP_ANH _cell_length_a 12.2967(15) _cell_length_b 17.7483(21) _cell_length_c 5.9887(8) _cell_angle_alpha 90.0 _cell_angle_beta 104.626(6) _cell_angle_gamma 90.0 _cell_volume 1264.7(4) _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21 1' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +x,+y,+z 2 -x,+y+1/2,-z # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity La La 0.6920(4) 0.25 0.3874(13) 1.0 Uiso 0.015 2 P P1 0.4447(12) 0.1314(15) 0.093(4) 1.0 Uiso 0.015 2 P P2 -0.2390(17) 0.1259(14) 0.929(5) 1.0 Uiso 0.015 2 O O1 0.4682(24) 0.1580(30) -0.135(6) 1.0 Uiso 0.015 2 O O2 0.4719(26) 0.1938(20) 0.276(7) 1.0 Uiso 0.015 2 O O3 0.5009(26) 0.0561(16) 0.175(7) 1.0 Uiso 0.015 2 O O4 -0.1116(18) 0.1117(25) 0.974(8) 1.0 Uiso 0.015 2 O O5 -0.2742(33) 0.1905(18) 0.752(8) 1.0 Uiso 0.015 2 O O6 -0.273(4) 0.1448(22) 1.153(7) 1.0 Uiso 0.015 2 C C1 0.2911(14) 0.1165(20) 0.031(7) 1.0 Uiso 0.015 2 C C2 -0.3124(31) 0.0416(16) 0.807(7) 1.0 Uiso 0.015 2 N N1 0.2365(20) 0.0646(14) 0.169(6) 1.0 Uiso 0.015 2 C C3 0.1424(32) 0.1049(21) 0.233(7) 1.0 Uiso 0.015 2 C C4 0.1156(33) 0.0760(29) 0.447(5) 1.0 Uiso 0.015 2 C C5 -0.0082(32) 0.063(4) 0.421(10) 1.0 Uiso 0.015 2 P P3 -0.4983(17) -0.1146(13) 0.803(4) 1.0 Uiso 0.015 2 P P4 0.2013(17) -0.1158(14) 0.061(5) 1.0 Uiso 0.015 2 O O1b -0.5298(32) -0.1312(32) 1.031(5) 1.0 Uiso 0.015 2 O O2b -0.5211(30) -0.1844(20) 0.644(8) 1.0 Uiso 0.015 2 O O3b -0.5611(26) -0.0446(18) 0.685(8) 1.0 Uiso 0.015 2 O O4b 0.0870(23) -0.1368(25) 0.101(7) 1.0 Uiso 0.015 2 O O5b 0.2957(28) -0.1502(24) 0.255(7) 1.0 Uiso 0.015 2 O O6b 0.2143(34) -0.1437(22) -0.175(6) 1.0 Uiso 0.015 2 C C1b -0.3488(18) -0.0964(19) 0.858(7) 1.0 Uiso 0.015 2 C C2b 0.217(4) -0.0147(14) 0.080(8) 1.0 Uiso 0.015 2 N N2 -0.3179(25) -0.0367(15) 0.706(5) 1.0 Uiso 0.015 2 C C8 -0.221(4) -0.0546(25) 0.604(9) 1.0 Uiso 0.015 2 C C7 -0.1248(33) 0.0004(34) 0.668(6) 1.0 Uiso 0.015 2 C C6 -0.036(4) -0.0061(30) 0.540(11) 1.0 Uiso 0.015 2 # If you change Z, be sure to change all 3 of the following _chemical_formula_sum 'C10 La N2 O12 H25 P4' _chemical_formula_weight 627.91 _cell_formula_units_Z 2 # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag La O2 2.802(30) . 1_555 N La O5 2.36(4) . 1_655 N La O6 2.439(24) . 1_654 N La P3 3.373(21) . 2_556 N La O2b 2.37(4) . 2_556 N La O5b 2.75(4) . 2_656 N La O6b 2.694(23) . 2_655 N P1 O1 1.543(6) . 1_555 N P1 O2 1.533(6) . 1_555 N P1 O3 1.527(6) . 1_555 N P1 C1 1.851(10) . 1_555 N P2 O4 1.541(6) . 1_555 N P2 O5 1.547(6) . 1_555 N P2 O6 1.542(6) . 1_555 N P2 C2 1.804(6) . 1_555 N O1 P1 1.543(6) . 1_555 N O2 La 2.802(30) . 1_555 N O2 P1 1.533(6) . 1_555 N O3 P1 1.527(6) . 1_555 N O4 P2 1.541(6) . 1_555 N O5 La 2.36(4) . 1_455 N O5 P2 1.547(6) . 1_555 N O6 La 2.439(24) . 1_456 N O6 P2 1.542(6) . 1_555 N C1 P1 1.851(10) . 1_555 N C1 N1 1.504(6) . 1_555 N C2 P2 1.804(6) . 1_555 N C2 N2 1.509(6) . 1_555 N N1 C1 1.504(6) . 1_555 N N1 C3 1.489(6) . 1_555 N N1 C2b 1.501(6) . 1_555 N C3 N1 1.489(6) . 1_555 N C3 C4 1.495(6) . 1_555 N C4 C3 1.495(6) . 1_555 N C4 C5 1.508(6) . 1_555 N C5 C4 1.508(6) . 1_555 N C5 C6 1.500(6) . 1_555 N P3 La 3.373(21) . 2_546 N P3 O1b 1.540(6) . 1_555 N P3 O2b 1.542(6) . 1_555 N P3 O3b 1.538(6) . 1_555 N P3 C1b 1.813(6) . 1_555 N P4 O4b 1.532(6) . 1_555 N P4 O5b 1.547(6) . 1_555 N P4 O6b 1.540(6) . 1_555 N P4 C2b 1.806(6) . 1_555 N O1b P3 1.540(6) . 1_555 N O2b La 2.37(4) . 2_546 N O2b P3 1.542(6) . 1_555 N O3b P3 1.538(6) . 1_555 N O4b P4 1.532(6) . 1_555 N O5b La 2.75(4) . 2_646 N O5b P4 1.547(6) . 1_555 N O6b La 2.694(23) . 2_645 N O6b P4 1.540(6) . 1_555 N C1b P3 1.813(6) . 1_555 N C1b N2 1.507(6) . 1_555 N C2b N1 1.501(6) . 1_555 N C2b P4 1.806(6) . 1_555 N N2 C2 1.509(6) . 1_555 N N2 C1b 1.507(6) . 1_555 N N2 C8 1.505(6) . 1_555 N C8 N2 1.505(6) . 1_555 N C8 C7 1.506(6) . 1_555 N C7 C8 1.506(6) . 1_555 N C7 C6 1.494(6) . 1_555 N C6 C5 1.500(6) . 1_555 N C6 C7 1.494(6) . 1_555 N loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 La O6 100.0(10) 1_655 . 1_654 N O5 La O2b 103.9(15) 1_655 . 2_556 N O5 La O5b 66.9(10) 1_655 . 2_656 N O5 La O6b 138.8(12) 1_655 . 2_655 N O6 La O2b 127.9(15) 1_654 . 2_556 N O6 La O5b 163.1(12) 1_654 . 2_656 N O6 La O6b 96.0(10) 1_654 . 2_655 N O2b La O5b 67.6(15) 2_556 . 2_656 N O2b La O6b 95.4(11) 2_556 . 2_655 N O5b La O6b 88.3(9) 2_656 . 2_655 N O1 P1 O2 110.9(8) 1_555 . 1_555 N O1 P1 O3 112.4(8) 1_555 . 1_555 N O1 P1 C1 106.1(8) 1_555 . 1_555 N O2 P1 O3 113.8(8) 1_555 . 1_555 N O2 P1 C1 105.9(7) 1_555 . 1_555 N O3 P1 C1 107.2(8) 1_555 . 1_555 N O4 P2 O5 109.9(8) 1_555 . 1_555 N O4 P2 O6 111.4(8) 1_555 . 1_555 N O4 P2 C2 108.6(7) 1_555 . 1_555 N O5 P2 O6 110.2(8) 1_555 . 1_555 N O5 P2 C2 108.3(7) 1_555 . 1_555 N O6 P2 C2 108.4(7) 1_555 . 1_555 N La O5 P2 156.4(24) 1_455 . 1_555 N La O6 P2 142.6(21) 1_456 . 1_555 N P1 C1 N1 123.5(19) 1_555 . 1_555 N P2 C2 N2 153.2(22) 1_555 . 1_555 N C1 N1 C3 109.2(9) 1_555 . 1_555 N C1 N1 C2b 115.6(10) 1_555 . 1_555 N C3 N1 C2b 118.4(11) 1_555 . 1_555 N N1 C3 C4 114.1(7) 1_555 . 1_555 N C3 C4 C5 113.4(10) 1_555 . 1_555 N C4 C5 C6 114.7(10) 1_555 . 1_555 N O1b P3 O2b 110.2(8) 1_555 . 1_555 N O1b P3 O3b 110.8(8) 1_555 . 1_555 N O1b P3 C1b 110.0(7) 1_555 . 1_555 N O2b P3 O3b 111.9(8) 1_555 . 1_555 N O2b P3 C1b 105.8(7) 1_555 . 1_555 N O3b P3 C1b 107.9(7) 1_555 . 1_555 N O4b P4 O5b 109.2(8) 1_555 . 1_555 N O4b P4 O6b 112.2(8) 1_555 . 1_555 N O4b P4 C2b 108.6(7) 1_555 . 1_555 N O5b P4 O6b 109.3(8) 1_555 . 1_555 N O5b P4 C2b 107.2(7) 1_555 . 1_555 N O6b P4 C2b 110.2(7) 1_555 . 1_555 N La O2b P3 117.6(20) 2_546 . 1_555 N La O5b P4 136.3(19) 2_646 . 1_555 N La O6b P4 144.5(21) 2_645 . 1_555 N P3 C1b N2 114.4(18) 1_555 . 1_555 N N1 C2b P4 163.5(27) 1_555 . 1_555 N C2 N2 C1b 113.5(10) 1_555 . 1_555 N C2 N2 C8 113.4(9) 1_555 . 1_555 N C1b N2 C8 116.3(10) 1_555 . 1_555 N N2 C8 C7 114.2(10) 1_555 . 1_555 N C8 C7 C6 116.7(10) 1_555 . 1_555 N C5 C6 C7 117.8(10) 1_555 . 1_555 N # Powder diffraction data for histogram 1 #============================================================================== # 9. INSTRUMENT CHARACTERIZATION _exptl_special_details ; ? ; # if regions of the data are excluded, the reason(s) are supplied here: _pd_proc_info_excluded_regions ; ? ; # The following item is used to identify the equipment used to record # the powder pattern when the diffractogram was measured at a laboratory # other than the authors' home institution, e.g. when neutron or synchrotron # radiation is used. _pd_instr_location ; ? ; _pd_calibration_special_details # description of the method used # to calibrate the instrument ; ? ; _diffrn_ambient_temperature 473 _diffrn_source ? _diffrn_source_target ? _diffrn_source_type ? _diffrn_measurement_device_type ? _diffrn_detector ? _diffrn_detector_type ? # make or model of detector _pd_meas_scan_method ? # options are 'step', 'cont', # 'tof', 'fixed' or # 'disp' (= dispersive) _pd_meas_special_details ; ? ; # The following two items identify the program(s) used (if appropriate). _computing_data_collection ? _computing_data_reduction ? # Describe any processing performed on the data, prior to refinement. # For example: a manual Lp correction or a precomputed absorption correction _pd_proc_info_data_reduction ? # The following item is used for angular dispersive measurements only. _diffrn_radiation_monochromator ? # The following items are used to define the size of the instrument. # Not all distances are appropriate for all instrument types. _pd_instr_dist_src/mono ? _pd_instr_dist_mono/spec ? _pd_instr_dist_src/spec ? _pd_instr_dist_spec/anal ? _pd_instr_dist_anal/detc ? _pd_instr_dist_spec/detc ? # 10. Specimen size and mounting information # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial ? # perpendicular to # equatorial plane _pd_spec_size_equat ? # parallel to # scattering vector # in transmission _pd_spec_size_thick ? # parallel to # scattering vector # in reflection _pd_spec_mounting # This field should be # used to give details of the # container. ; ? ; _pd_spec_mount_mode ? # options are 'reflection' # or 'transmission' _pd_spec_shape ? # options are 'cylinder' # 'flat_sheet' or 'irregular' loop_ _atom_type_symbol _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source La 2.0 0.000 0.000 20.5780 2.94817 19.5990 0.24448 11.3727 18.7726 3.28719 133.124 2.14678 International_Tables_Vol_C P 8.0 0.000 0.000 6.43450 1.90670 4.17910 27.1570 1.78000 0.52600 1.49080 68.1645 1.11490 International_Tables_Vol_C O 24.0 0.000 0.000 3.04850 13.2771 2.28680 5.70110 1.54630 0.32390 0.86700 32.9089 0.25080 International_Tables_Vol_C C 20.0 0.000 0.000 2.31000 20.8439 1.02000 10.2075 1.58860 0.56870 0.86500 51.6512 0.21560 International_Tables_Vol_C N 4.0 0.000 0.000 12.2126 0.00570 3.13220 9.89330 2.01250 28.9975 1.16630 0.58260 -11.529 International_Tables_Vol_C _diffrn_radiation_probe x-ray _diffrn_radiation_polarisn_ratio ? _diffrn_radiation_wavelength 1.5406 _diffrn_radiation_type ? _pd_proc_ls_prof_R_factor 0.0604 _pd_proc_ls_prof_wR_factor 0.0812 _pd_proc_ls_prof_wR_expected 0.0304 _refine_ls_R_Fsqd_factor 0.11687 _pd_proc_ls_background_function ; GSAS Background function number 1 with 10 terms. Shifted Chebyshev function of 1st kind 1: 772.003 2: -487.642 3: 200.742 4: -71.4941 5: 36.4576 6: -47.6843 7: 29.5909 8: -46.5627 9: 46.7672 10: -47.0939 ; _exptl_absorpt_process_details ; GSAS Absorption/surface roughness correction: function number 0 No correction is applied. ; _exptl_absorpt_correction_T_min 1.00000 _exptl_absorpt_correction_T_max 1.00000 _pd_proc_ls_profile_function ; CW Profile function number 3 with 19 terms Pseudovoigt profile coefficients as parameterized in P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. Asymmetry correction of L.W. Finger, D.E. Cox & A. P. Jephcoat (1994). J. Appl. Cryst.,27,892-900. #1(GU) = 0.000 #2(GV) = 0.000 #3(GW) = 8.440 #4(GP) = 0.000 #5(LX) = 0.000 #6(LY) = 93.492 #7(S/L) = 0.0132 #8(H/L) = 0.0141 #9(trns) = 0.00 #10(shft)= 0.0000 #11(stec)= -31.86 #12(ptec)= 0.00 #13(sfec)= 0.00 #14(L11) = 0.000 #15(L22) = 0.000 #16(L33) = 0.000 #17(L12) = 0.000 #18(L13) = 0.000 #19(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0050 times the peak Aniso. broadening axis 0.0 0.0 1.0 ; _pd_proc_ls_peak_cutoff 0.00500 _pd_proc_info_datetime 2011-12-08T19:32:12 _pd_calc_method 'Rietveld Refinement' #---- raw/calc data loop ----- _pd_meas_2theta_range_min 4.308 _pd_meas_2theta_range_max 100.29 _pd_meas_2theta_range_inc 0.017 _pd_proc_2theta_range_min 4.27944 _pd_proc_2theta_range_max 100.26144 _pd_proc_2theta_range_inc 0.017 _reflns_number_total 1072 _reflns_limit_h_min 0 _reflns_limit_h_max 11 _reflns_limit_k_min 0 _reflns_limit_k_max 17 _reflns_limit_l_min -5 _reflns_limit_l_max 5 _reflns_d_resolution_high 1.090 _reflns_d_resolution_low 5.949 #--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--# # Attachment 'web_deposit_cif_file_1_RosarioMPerezColodrero_1323857331.LaH5DTMP7H2O.cif' data_LAH5DTMP.7H2O_publ _database_code_depnum_ccdc_archive 'CCDC 810316' #TrackingRef 'web_deposit_cif_file_1_RosarioMPerezColodrero_1323857331.LaH5DTMP7H2O.cif' _ccdc_journal_manuscript_code DT-ART-10-2011-01199 _pd_block_id 2011-12-08T10:18|LAH5DTMP.7H20|LaH5DTMP.7H2O_ID31|X'Pert_Pro _audit_creation_method 'from EXP file using GSAS2CIF' _audit_creation_date 2011-12-08T10:18 _audit_author_name LaHDTMP_ID31 _audit_update_record ; 2011-12-08T10:18 Initial CIF as created by GSAS2CIF ; _publ_section_title_footnote ; ? ; #============================================================================== # 4. TEXT _publ_section_synopsis ; ? ; _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_exptl_prep # Details of the preparation of the sample(s) # should be given here. ; ? ; _publ_section_exptl_refinement ; ? ; _publ_section_references ; ? ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; #============================================================================= # 5. OVERALL REFINEMENT & COMPUTING DETAILS _refine_special_details ; ? ; _pd_proc_ls_special_details ; ? ; # The following items are used to identify the programs used. _computing_molecular_graphics ? _computing_publication_material ? _refine_ls_weighting_scheme ? _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_number_constraints ? _refine_ls_restrained_S_all ? _refine_ls_restrained_S_obs ? #============================================================================== # 6. SAMPLE PREPARATION DATA # (In the unusual case where multiple samples are used in a single # Rietveld study, this information should be moved into the phase # blocks) # The following three fields describe the preparation of the material. # The cooling rate is in K/min. The pressure at which the sample was # prepared is in kPa. The temperature of preparation is in K. _pd_prep_cool_rate ? _pd_prep_pressure ? _pd_prep_temperature ? _pd_char_colour ? # use ICDD colour descriptions _refine_ls_shift/su_max 0.05 _refine_ls_shift/su_mean 0.02 _computing_structure_refinement GSAS _refine_ls_number_parameters 139 _refine_ls_goodness_of_fit_all 2.75 _refine_ls_number_restraints 68 _refine_ls_matrix_type full #============================================================================== # 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA _pd_char_particle_morphology ? _chemical_name_systematic ; ? ; _chemical_name_common LaH5DTMP.7H2O _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_melting_point ? _chemical_compound_source ? # for minerals and # natural products _symmetry_space_group_name_Hall ? _exptl_crystal_F_000 ? _exptl_crystal_density_diffrn ? _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _cell_measurement_temperature ? _cell_special_details ; ? ; _geom_special_details ? # The following item identifies the program(s) used (if appropriate). _computing_structure_solution ? #============================================================================== # 8. Phase information from GSAS _pd_phase_name LaH5DTMP.7H2O _cell_length_a 13.3444(5) _cell_length_b 18.7820(4) _cell_length_c 5.84903(23) _cell_angle_alpha 90.0 _cell_angle_beta 97.711(4) _cell_angle_gamma 90.0 _cell_volume 1452.71(10) _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21 1' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +x,+y,+z 2 -x,+y+1/2,-z # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity La La 0.6289(4) 0.25 0.3351(9) 1.0 Uiso 0.0274(23) 2 P P1 0.4399(25) 0.0853(13) 0.144(4) 1.0 Uiso 0.023(5) 2 P P2 -0.2669(23) 0.1336(9) 0.863(4) 1.0 Uiso 0.023(5) 2 O O1 0.423(4) 0.0743(22) -0.119(4) 1.0 Uiso 0.041(5) 2 O O2 0.463(4) 0.1636(15) 0.206(8) 1.0 Uiso 0.041(5) 2 O O3 0.5249(34) 0.0366(23) 0.258(7) 1.0 Uiso 0.041(5) 2 O O4 -0.1574(24) 0.1380(18) 0.807(7) 1.0 Uiso 0.041(5) 2 O O5 -0.3390(28) 0.1758(18) 0.684(6) 1.0 Uiso 0.041(5) 2 O O6 -0.271(4) 0.1613(17) 1.109(4) 1.0 Uiso 0.041(5) 2 C C1 0.3248(33) 0.0624(25) 0.261(8) 1.0 Uiso 0.041(5) 2 C C2 -0.306(4) 0.0417(11) 0.845(8) 1.0 Uiso 0.041(5) 2 N N1 0.2674(25) -0.0073(19) 0.249(6) 1.0 Uiso 0.041(5) 2 C C3 0.1643(23) 0.0055(24) 0.318(6) 1.0 Uiso 0.041(5) 2 C C4 0.1550(29) -0.0187(29) 0.558(5) 1.0 Uiso 0.041(5) 2 C C5 0.0470(32) -0.0215(27) 0.604(7) 1.0 Uiso 0.041(5) 2 O Ow1 0.5082(33) 0.2257(23) 0.806(7) 1.0 Uiso 0.041(5) 2 O Ow2 0.1304(34) 0.2284(19) 0.554(8) 1.0 Uiso 0.041(5) 2 O Ow3 0.094(4) 0.1623(25) 0.887(9) 1.0 Uiso 0.041(5) 2 O Ow4 1.0224(33) 0.3074(20) 0.170(8) 1.0 Uiso 0.041(5) 2 O Ow5 0.9022(32) 0.2250(24) 0.442(7) 1.0 Uiso 0.041(5) 2 O Ow6 0.210(4) 0.2219(20) 0.124(7) 1.0 Uiso 0.041(5) 2 P P3 -0.4576(21) -0.0955(11) 0.780(4) 1.0 Uiso 0.023(5) 2 P P4 0.2803(19) -0.1349(10) 0.1063(33) 1.0 Uiso 0.023(5) 2 O O1b -0.437(4) -0.0909(22) 1.045(4) 1.0 Uiso 0.041(5) 2 O O2b -0.4967(32) -0.1696(16) 0.700(7) 1.0 Uiso 0.041(5) 2 O O3b -0.5338(31) -0.0376(22) 0.684(8) 1.0 Uiso 0.041(5) 2 O O4b 0.1731(20) -0.1674(20) 0.080(6) 1.0 Uiso 0.041(5) 2 O O5b 0.3308(30) -0.1372(18) 0.358(4) 1.0 Uiso 0.041(5) 2 O O6b 0.3474(27) -0.1716(17) -0.052(6) 1.0 Uiso 0.041(5) 2 C C1b -0.3403(29) -0.0793(18) 0.664(8) 1.0 Uiso 0.041(5) 2 C C2b 0.266(4) -0.0429(11) 0.018(6) 1.0 Uiso 0.041(5) 2 N N2 -0.2817(23) -0.0103(16) 0.663(5) 1.0 Uiso 0.041(5) 2 C C8 -0.1704(22) -0.0183(26) 0.649(6) 1.0 Uiso 0.041(5) 2 C C7 -0.1374(32) -0.0192(28) 0.415(7) 1.0 Uiso 0.041(5) 2 C C6 -0.0303(31) -0.0413(26) 0.404(10) 1.0 Uiso 0.041(5) 2 O Ow7 -0.172(4) -0.1532(23) -0.874(8) 1.0 Uiso 0.041(5) 2 # If you change Z, be sure to change all 3 of the following _chemical_formula_sum 'C10 La N2 O19 H39 P4' _chemical_formula_weight 753.91 _cell_formula_units_Z 2 # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag La O2 2.768(35) . 1_555 N La O5 2.461(32) . 1_655 N La O6 2.602(31) . 1_654 N La O2b 2.310(24) . 2_556 N La O5b 2.782(29) . 2_656 N La O6b 2.271(22) . 2_655 N P1 O1 1.538(6) . 1_555 N P1 O2 1.536(6) . 1_555 N P1 O3 1.540(6) . 1_555 N P1 C1 1.817(6) . 1_555 N P2 O4 1.543(6) . 1_555 N P2 O5 1.543(6) . 1_555 N P2 O6 1.536(6) . 1_555 N P2 C2 1.801(4) . 1_555 N O1 P1 1.538(6) . 1_555 N O2 La 2.768(35) . 1_555 N O2 P1 1.536(6) . 1_555 N O3 P1 1.540(6) . 1_555 N O4 P2 1.543(6) . 1_555 N O5 La 2.461(32) . 1_455 N O5 P2 1.543(6) . 1_555 N O6 La 2.602(31) . 1_456 N O6 P2 1.536(6) . 1_555 N C1 P1 1.817(6) . 1_555 N C1 N1 1.513(6) . 1_555 N C2 P2 1.801(4) . 1_555 N C2 N2 1.510(6) . 1_555 N N1 C1 1.513(6) . 1_555 N N1 C3 1.503(6) . 1_555 N N1 P4 2.552(33) . 1_555 N N1 C2b 1.509(6) . 1_555 N C3 N1 1.503(6) . 1_555 N C3 C4 1.495(6) . 1_555 N C4 C3 1.495(6) . 1_555 N C4 C5 1.503(6) . 1_555 N C5 C4 1.503(6) . 1_555 N C5 C6 1.500(6) . 1_555 N P3 O1b 1.538(6) . 1_555 N P3 O2b 1.537(6) . 1_555 N P3 O3b 1.543(6) . 1_555 N P3 C1b 1.815(6) . 1_555 N P4 N1 2.552(33) . 1_555 N P4 O4b 1.543(6) . 1_555 N P4 O5b 1.535(6) . 1_555 N P4 O6b 1.534(6) . 1_555 N P4 C2b 1.807(6) . 1_555 N O1b P3 1.538(6) . 1_555 N O2b La 2.310(24) . 2_546 N O2b P3 1.537(6) . 1_555 N O3b P3 1.543(6) . 1_555 N O4b P4 1.543(6) . 1_555 N O5b La 2.782(29) . 2_646 N O5b P4 1.535(6) . 1_555 N O6b La 2.271(22) . 2_645 N O6b P4 1.534(6) . 1_555 N C1b P3 1.815(6) . 1_555 N C1b N2 1.513(6) . 1_555 N C2b N1 1.509(6) . 1_555 N C2b P4 1.807(6) . 1_555 N N2 C2 1.510(6) . 1_555 N N2 C1b 1.513(6) . 1_555 N N2 C8 1.506(6) . 1_555 N C8 N2 1.506(6) . 1_555 N C8 C7 1.495(6) . 1_555 N C7 C8 1.495(6) . 1_555 N C7 C6 1.498(6) . 1_555 N C6 C5 1.500(6) . 1_555 N C6 C7 1.498(6) . 1_555 N loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 La O5 86.5(12) 1_555 . 1_655 N O2 La O6 86.1(11) 1_555 . 1_654 N O2 La O2b 77.6(9) 1_555 . 2_556 N O2 La O6b 111.4(14) 1_555 . 2_655 N O5 La O6 90.9(9) 1_655 . 1_654 N O5 La O2b 119.4(13) 1_655 . 2_556 N O5 La O6b 161.2(12) 1_655 . 2_655 N O6 La O2b 144.0(14) 1_654 . 2_556 N O6 La O6b 85.0(9) 1_654 . 2_655 N O2b La O6b 71.9(11) 2_556 . 2_655 N O1 P1 O2 111.4(8) 1_555 . 1_555 N O1 P1 O3 110.8(8) 1_555 . 1_555 N O1 P1 C1 109.2(7) 1_555 . 1_555 N O2 P1 O3 110.7(8) 1_555 . 1_555 N O2 P1 C1 106.8(7) 1_555 . 1_555 N O3 P1 C1 107.8(7) 1_555 . 1_555 N O4 P2 O5 110.4(8) 1_555 . 1_555 N O4 P2 O6 109.8(8) 1_555 . 1_555 N O4 P2 C2 108.1(7) 1_555 . 1_555 N O5 P2 O6 111.3(8) 1_555 . 1_555 N O5 P2 C2 107.7(7) 1_555 . 1_555 N O6 P2 C2 109.5(7) 1_555 . 1_555 N La O2 P1 138.8(22) 1_555 . 1_555 N La O5 P2 151.4(23) 1_455 . 1_555 N La O6 P2 141.1(22) 1_456 . 1_555 N P1 C1 N1 129.5(22) 1_555 . 1_555 N P2 C2 N2 125.2(19) 1_555 . 1_555 N C1 N1 C3 109.0(9) 1_555 . 1_555 N C1 N1 C2b 111.7(9) 1_555 . 1_555 N C3 N1 C2b 114.1(10) 1_555 . 1_555 N N1 C3 C4 113.4(7) 1_555 . 1_555 N C3 C4 C5 112.5(9) 1_555 . 1_555 N C4 C5 C6 116.4(10) 1_555 . 1_555 N O1b P3 O2b 111.4(8) 1_555 . 1_555 N O1b P3 O3b 110.4(8) 1_555 . 1_555 N O1b P3 C1b 108.9(7) 1_555 . 1_555 N O2b P3 O3b 110.2(8) 1_555 . 1_555 N O2b P3 C1b 108.2(7) 1_555 . 1_555 N O3b P3 C1b 107.6(7) 1_555 . 1_555 N O4b P4 O5b 111.6(8) 1_555 . 1_555 N O4b P4 O6b 111.7(8) 1_555 . 1_555 N O4b P4 C2b 106.7(7) 1_555 . 1_555 N O5b P4 O6b 110.4(8) 1_555 . 1_555 N O5b P4 C2b 108.6(7) 1_555 . 1_555 N O6b P4 C2b 107.7(7) 1_555 . 1_555 N La O2b P3 147.5(20) 2_546 . 1_555 N La O6b P4 151.7(20) 2_645 . 1_555 N P3 C1b N2 128.1(16) 1_555 . 1_555 N N1 C2b P4 100.2(18) 1_555 . 1_555 N C2 N2 C1b 113.2(9) 1_555 . 1_555 N C2 N2 C8 114.0(10) 1_555 . 1_555 N C1b N2 C8 115.4(10) 1_555 . 1_555 N N2 C8 C7 117.7(10) 1_555 . 1_555 N C8 C7 C6 116.3(10) 1_555 . 1_555 N C5 C6 C7 117.3(10) 1_555 . 1_555 N # Powder diffraction data for histogram 1 #============================================================================== # 9. INSTRUMENT CHARACTERIZATION _exptl_special_details ; ? ; # if regions of the data are excluded, the reason(s) are supplied here: _pd_proc_info_excluded_regions ; ? ; # The following item is used to identify the equipment used to record # the powder pattern when the diffractogram was measured at a laboratory # other than the authors' home institution, e.g. when neutron or synchrotron # radiation is used. _pd_instr_location ; ? ; _pd_calibration_special_details # description of the method used # to calibrate the instrument ; ? ; _diffrn_ambient_temperature 293 _diffrn_source ? _diffrn_source_target ? _diffrn_source_type ? _diffrn_measurement_device_type ? _diffrn_detector ? _diffrn_detector_type ? # make or model of detector _pd_meas_scan_method ? # options are 'step', 'cont', # 'tof', 'fixed' or # 'disp' (= dispersive) _pd_meas_special_details ; ? ; # The following two items identify the program(s) used (if appropriate). _computing_data_collection ? _computing_data_reduction ? # Describe any processing performed on the data, prior to refinement. # For example: a manual Lp correction or a precomputed absorption correction _pd_proc_info_data_reduction ? # The following item is used for angular dispersive measurements only. _diffrn_radiation_monochromator ? # The following items are used to define the size of the instrument. # Not all distances are appropriate for all instrument types. _pd_instr_dist_src/mono ? _pd_instr_dist_mono/spec ? _pd_instr_dist_src/spec ? _pd_instr_dist_spec/anal ? _pd_instr_dist_anal/detc ? _pd_instr_dist_spec/detc ? # 10. Specimen size and mounting information # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial ? # perpendicular to # equatorial plane _pd_spec_size_equat ? # parallel to # scattering vector # in transmission _pd_spec_size_thick ? # parallel to # scattering vector # in reflection _pd_spec_mounting # This field should be # used to give details of the # container. ; ? ; _pd_spec_mount_mode ? # options are 'reflection' # or 'transmission' _pd_spec_shape ? # options are 'cylinder' # 'flat_sheet' or 'irregular' loop_ _atom_type_symbol _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source La 2.0 -2.214 3.142 20.5780 2.94817 19.5990 0.24448 11.3727 18.7726 3.28719 133.124 2.14678 International_Tables_Vol_C P 8.0 0.001 0.016 6.43450 1.90670 4.17910 27.1570 1.78000 0.52600 1.49080 68.1645 1.11490 International_Tables_Vol_C O 38.0 -0.004 0.001 3.04850 13.2771 2.28680 5.70110 1.54630 0.32390 0.86700 32.9089 0.25080 International_Tables_Vol_C C 20.0 -0.002 0.000 2.31000 20.8439 1.02000 10.2075 1.58860 0.56870 0.86500 51.6512 0.21560 International_Tables_Vol_C N 4.0 -0.003 0.000 12.2126 0.00570 3.13220 9.89330 2.01250 28.9975 1.16630 0.58260 -11.529 International_Tables_Vol_C _diffrn_radiation_probe x-ray _diffrn_radiation_polarisn_ratio ? _diffrn_radiation_wavelength 0.2998 _diffrn_radiation_type ? _pd_proc_ls_prof_R_factor 0.0532 _pd_proc_ls_prof_wR_factor 0.0741 _pd_proc_ls_prof_wR_expected 0.0277 _refine_ls_R_Fsqd_factor 0.09562 _pd_proc_ls_background_function ; GSAS Background function number 1 with 15 terms. Shifted Chebyshev function of 1st kind 1: 893.287 2: -28.3582 3: -20.2483 4: 45.2373 5: 11.4761 6: -3.56504 7: -6.62751 8: 9.76445 9: -22.5774 10: 25.6377 11: -20.5662 12: -12.6433 13: 21.6981 14: 1.75725 15: -11.1126 ; _exptl_absorpt_process_details ; GSAS Absorption/surface roughness correction: function number 0 No correction is applied. ; _exptl_absorpt_correction_T_min 1.00000 _exptl_absorpt_correction_T_max 1.00000 _pd_proc_ls_pref_orient_corr ; March-Dollase AXIS 1 Ratio= 1.14871 h= 1.000 k= 0.000 l= 0.000 Prefered orientation correction range: Min= 0.65979, Max= 1.23111 ; _pd_proc_ls_profile_function ; CW Profile function number 4 with 21 terms Pseudovoigt profile coefficients as parameterized in P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. Asymmetry correction of L.W. Finger, D.E. Cox & A. P. Jephcoat (1994). J. Appl. Cryst.,27,892-900. Microstrain broadening by P.W. Stephens, (1999). J. Appl. Cryst.,32,281-289. #1(GU) = 0.000 #2(GV) = 0.000 #3(GW) = 0.171 #4(GP) = 0.000 #5(LX) = 0.205 #6(ptec) = 0.00 #7(trns) = 0.00 #8(shft) = 0.0000 #9(sfec) = 0.00 #10(S/L) = 0.0011 #11(H/L) = 0.0008 #12(eta) = 0.5741 #13(S400 ) = 6.3E-02 #14(S040 ) = 1.2E-03 #15(S004 ) = 2.9E+00 #16(S220 ) = 9.3E-03 #17(S202 ) = 1.0E+00 #18(S022 ) = -1.2E-02 #19(S301 ) = 4.0E-01 #20(S103 ) = 1.6E+00 #21(S121 ) = 2.2E-03 Peak tails are ignored where the intensity is below 0.0030 times the peak Aniso. broadening axis 0.0 0.0 1.0 ; _pd_proc_ls_peak_cutoff 0.00300 _pd_proc_info_datetime 2011-12-08T10:18:10 _pd_calc_method 'Rietveld Refinement' #---- raw/calc data loop ----- _pd_meas_2theta_range_min 0.003 _pd_meas_2theta_range_max 33.0 _pd_meas_2theta_range_inc 0.003 _pd_proc_2theta_range_min 0.001492 _pd_proc_2theta_range_max 32.998493 _pd_proc_2theta_range_inc 0.003 _reflns_number_total 1041 _reflns_limit_h_min 0 _reflns_limit_h_max 11 _reflns_limit_k_min 0 _reflns_limit_k_max 16 _reflns_limit_l_min -5 _reflns_limit_l_max 5 _reflns_d_resolution_high 1.149 _reflns_d_resolution_low 13.224 #--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--# # Attachment 'web_deposit_cif_file_2_RosarioMPerezColodrero_1323857331.LAHDTMP.2H2O.cif' data_LAH5DTMP.2H2O_publ _database_code_depnum_ccdc_archive 'CCDC 810317' #TrackingRef 'web_deposit_cif_file_2_RosarioMPerezColodrero_1323857331.LAHDTMP.2H2O.cif' _ccdc_journal_manuscript_code DT-ART-10-2011-01199 _pd_block_id 2011-12-08T13:21|LAH5DTMP.2H2O|LAH5DTMP.2H2O|X'Pert_Pro _audit_creation_method 'from EXP file using GSAS2CIF' _audit_creation_date 2011-12-08T13:21 _audit_author_name LaHDTMP_ID31 _audit_update_record ; 2011-12-08T13:21 Initial CIF as created by GSAS2CIF ; _publ_section_title_footnote ; ? ; #============================================================================== # 4. TEXT _publ_section_synopsis ; ? ; _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_exptl_prep # Details of the preparation of the sample(s) # should be given here. ; ? ; _publ_section_exptl_refinement ; ? ; _publ_section_references ; ? ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; #============================================================================= # 5. OVERALL REFINEMENT & COMPUTING DETAILS _refine_special_details ; ? ; _pd_proc_ls_special_details ; ? ; # The following items are used to identify the programs used. _computing_molecular_graphics ? _computing_publication_material ? _refine_ls_weighting_scheme ? _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_number_constraints ? _refine_ls_restrained_S_all ? _refine_ls_restrained_S_obs ? #============================================================================== # 6. SAMPLE PREPARATION DATA # (In the unusual case where multiple samples are used in a single # Rietveld study, this information should be moved into the phase # blocks) # The following three fields describe the preparation of the material. # The cooling rate is in K/min. The pressure at which the sample was # prepared is in kPa. The temperature of preparation is in K. _pd_prep_cool_rate ? _pd_prep_pressure ? _pd_prep_temperature ? _pd_char_colour ? # use ICDD colour descriptions _refine_ls_shift/su_max 0.08 _refine_ls_shift/su_mean 0.01 _computing_structure_refinement GSAS _refine_ls_number_parameters 127 _refine_ls_goodness_of_fit_all 4.52 _refine_ls_number_restraints 74 _refine_ls_matrix_type full #============================================================================== # 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA _pd_char_particle_morphology ? _chemical_name_systematic ; ? ; _chemical_name_common LaH5DTMP.2H2O _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_melting_point ? _chemical_compound_source ? # for minerals and # natural products _symmetry_space_group_name_Hall ? _exptl_crystal_F_000 ? _exptl_crystal_density_diffrn ? _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _cell_measurement_temperature 293 _cell_special_details ; ? ; _geom_special_details ? # The following item identifies the program(s) used (if appropriate). _computing_structure_solution ? #============================================================================== # 8. Phase information from GSAS _pd_phase_name LaH5DTMP.2H2O _cell_length_a 12.5035(6) _cell_length_b 18.1874(10) _cell_length_c 5.82000(33) _cell_angle_alpha 90.0 _cell_angle_beta 101.923(4) _cell_angle_gamma 90.0 _cell_volume 1294.95(11) _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21 1' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +x,+y,+z 2 -x,+y+1/2,-z # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity La La 0.6695(4) 0.25 0.3763(11) 1.0 Uiso 0.01 2 P P1 0.4652(16) 0.0889(13) 0.180(5) 1.0 Uiso 0.01 2 P P2 -0.2521(14) 0.1126(11) 0.914(4) 1.0 Uiso 0.01 2 O O1 0.4299(30) 0.0892(24) -0.086(5) 1.0 Uiso 0.01 2 O O2 0.4996(22) 0.1682(16) 0.259(8) 1.0 Uiso 0.01 2 O O3 0.5493(26) 0.0301(19) 0.278(8) 1.0 Uiso 0.01 2 O O4 -0.1270(16) 0.1066(24) 0.931(9) 1.0 Uiso 0.01 2 O O5 -0.3049(35) 0.1630(20) 0.710(6) 1.0 Uiso 0.01 2 O O6 -0.2815(31) 0.1341(15) 1.151(5) 1.0 Uiso 0.01 2 C C1 0.3484(23) 0.0732(23) 0.319(7) 1.0 Uiso 0.01 2 C C2 -0.3091(33) 0.0229(14) 0.833(6) 1.0 Uiso 0.01 2 N N1 0.2429(19) 0.0320(16) 0.287(6) 1.0 Uiso 0.01 2 C C3 0.1529(28) 0.0878(23) 0.274(7) 1.0 Uiso 0.01 2 C C4 0.1237(30) 0.0992(24) 0.510(8) 1.0 Uiso 0.01 2 C C5 0.0166(34) 0.0652(25) 0.524(10) 1.0 Uiso 0.01 2 P P3 -0.4468(15) -0.1014(12) 0.797(5) 1.0 Uiso 0.01 2 P P4 0.2068(15) -0.1196(10) 0.073(4) 1.0 Uiso 0.01 2 O O1b -0.4326(30) -0.1341(22) 1.045(5) 1.0 Uiso 0.01 2 O O2b -0.5169(25) -0.1514(18) 0.602(6) 1.0 Uiso 0.01 2 O O3b -0.4922(27) -0.0241(15) 0.767(8) 1.0 Uiso 0.01 2 O O4b 0.0820(17) -0.1320(24) 0.041(8) 1.0 Uiso 0.01 2 O O5b 0.268(4) -0.1532(21) 0.306(6) 1.0 Uiso 0.01 2 O O6b 0.2484(31) -0.1513(19) -0.140(6) 1.0 Uiso 0.01 2 C C1b -0.3115(20) -0.1057(15) 0.721(8) 1.0 Uiso 0.01 2 C C2b 0.2312(34) -0.0217(10) 0.087(7) 1.0 Uiso 0.01 2 N N2 -0.3003(28) -0.0285(17) 0.636(6) 1.0 Uiso 0.01 2 C C8 -0.2093(33) -0.0137(26) 0.510(6) 1.0 Uiso 0.01 2 C C7 -0.0970(33) -0.0373(28) 0.643(10) 1.0 Uiso 0.01 2 C C6 -0.001(4) -0.0151(25) 0.541(13) 1.0 Uiso 0.01 2 O Ow1 0.0549(30) 0.257(5) 0.104(7) 1.0 Uiso 0.01 2 O Ow2 0.2776(29) 0.2722(29) 0.574(7) 1.0 Uiso 0.01 2 # If you change Z, be sure to change all 3 of the following _chemical_formula_sum 'C10 La N2 O14 H29 P4' _chemical_formula_weight 663.96 _cell_formula_units_Z 2 # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag La O2 2.568(16) . 1_555 N La O5 2.474(16) . 1_655 N La O6 2.623(17) . 1_654 N La O2b 2.640(17) . 2_556 N La O5b 2.556(16) . 2_656 N La O6b 2.599(16) . 2_655 N P1 O1 1.523(9) . 1_555 N P1 O2 1.547(9) . 1_555 N P1 O3 1.525(9) . 1_555 N P1 C1 1.829(16) . 1_555 N P2 O4 1.551(9) . 1_555 N P2 O5 1.536(9) . 1_555 N P2 O6 1.548(9) . 1_555 N P2 C2 1.804(9) . 1_555 N O1 P1 1.523(9) . 1_555 N O2 La 2.568(16) . 1_555 N O2 P1 1.547(9) . 1_555 N O3 P1 1.525(9) . 1_555 N O4 P2 1.551(9) . 1_555 N O5 La 2.474(16) . 1_455 N O5 P2 1.536(9) . 1_555 N O6 La 2.623(17) . 1_456 N O6 P2 1.548(9) . 1_555 N C1 P1 1.829(16) . 1_555 N C1 N1 1.494(10) . 1_555 N C2 P2 1.804(9) . 1_555 N C2 N2 1.498(10) . 1_555 N N1 C1 1.494(10) . 1_555 N N1 C3 1.506(10) . 1_555 N N1 C2b 1.502(10) . 1_555 N C3 N1 1.506(10) . 1_555 N C3 C4 1.508(10) . 1_555 N C4 C3 1.508(10) . 1_555 N C4 C5 1.492(10) . 1_555 N C5 C4 1.492(10) . 1_555 N C5 C6 1.483(10) . 1_555 N P3 O1b 1.536(9) . 1_555 N P3 O2b 1.570(9) . 1_555 N P3 O3b 1.513(9) . 1_555 N P3 C1b 1.836(9) . 1_555 N P4 O4b 1.549(9) . 1_555 N P4 O5b 1.539(9) . 1_555 N P4 O6b 1.551(9) . 1_555 N P4 C2b 1.805(9) . 1_555 N O1b P3 1.536(9) . 1_555 N O2b La 2.640(17) . 2_546 N O2b P3 1.570(9) . 1_555 N O3b P3 1.513(9) . 1_555 N O4b P4 1.549(9) . 1_555 N O5b La 2.556(16) . 2_646 N O5b P4 1.539(9) . 1_555 N O6b La 2.599(16) . 2_645 N O6b P4 1.551(9) . 1_555 N C1b P3 1.836(9) . 1_555 N C1b N2 1.504(10) . 1_555 N C2b N1 1.502(10) . 1_555 N C2b P4 1.805(9) . 1_555 N N2 C2 1.498(10) . 1_555 N N2 C1b 1.504(10) . 1_555 N N2 C8 1.500(10) . 1_555 N C8 N2 1.500(10) . 1_555 N C8 C7 1.519(10) . 1_555 N C7 C8 1.519(10) . 1_555 N C7 C6 1.504(10) . 1_555 N C6 C5 1.483(10) . 1_555 N C6 C7 1.504(10) . 1_555 N loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 La O5 78.7(13) 1_555 . 1_655 N O2 La O6 70.6(11) 1_555 . 1_654 N O2 La O2b 80.8(9) 1_555 . 2_556 N O2 La O5b 134.6(15) 1_555 . 2_656 N O2 La O6b 130.9(14) 1_555 . 2_655 N O5 La O6 82.7(8) 1_655 . 1_654 N O5 La O2b 112.0(14) 1_655 . 2_556 N O5 La O5b 84.3(10) 1_655 . 2_656 N O5 La O6b 148.9(14) 1_655 . 2_655 N O6 La O2b 144.6(11) 1_654 . 2_556 N O6 La O5b 148.1(13) 1_654 . 2_656 N O6 La O6b 97.5(9) 1_654 . 2_655 N O2b La O5b 67.2(12) 2_556 . 2_656 N O2b La O6b 85.7(11) 2_556 . 2_655 N O5b La O6b 79.3(7) 2_656 . 2_655 N O1 P1 O2 107.7(12) 1_555 . 1_555 N O1 P1 O3 114.6(13) 1_555 . 1_555 N O1 P1 C1 111.0(12) 1_555 . 1_555 N O2 P1 O3 114.5(13) 1_555 . 1_555 N O2 P1 C1 102.3(11) 1_555 . 1_555 N O3 P1 C1 106.1(12) 1_555 . 1_555 N O4 P2 O5 111.1(12) 1_555 . 1_555 N O4 P2 O6 112.4(12) 1_555 . 1_555 N O4 P2 C2 107.0(11) 1_555 . 1_555 N O5 P2 O6 113.2(12) 1_555 . 1_555 N O5 P2 C2 104.8(11) 1_555 . 1_555 N O6 P2 C2 107.9(11) 1_555 . 1_555 N La O2 P1 141.5(18) 1_555 . 1_555 N La O5 P2 162.4(26) 1_455 . 1_555 N La O6 P2 140.5(19) 1_456 . 1_555 N P1 C1 N1 142.0(21) 1_555 . 1_555 N P2 C2 N2 132.5(21) 1_555 . 1_555 N C1 N1 C3 107.5(14) 1_555 . 1_555 N C1 N1 C2b 111.4(14) 1_555 . 1_555 N C3 N1 C2b 116.7(16) 1_555 . 1_555 N N1 C3 C4 111.7(10) 1_555 . 1_555 N C3 C4 C5 112.4(12) 1_555 . 1_555 N C4 C5 C6 123.8(18) 1_555 . 1_555 N O1b P3 O2b 113.0(12) 1_555 . 1_555 N O1b P3 O3b 115.9(13) 1_555 . 1_555 N O1b P3 C1b 105.9(11) 1_555 . 1_555 N O2b P3 O3b 108.3(12) 1_555 . 1_555 N O2b P3 C1b 101.9(10) 1_555 . 1_555 N O3b P3 C1b 110.7(11) 1_555 . 1_555 N O4b P4 O5b 110.9(12) 1_555 . 1_555 N O4b P4 O6b 110.3(12) 1_555 . 1_555 N O4b P4 C2b 107.8(11) 1_555 . 1_555 N O5b P4 O6b 111.4(12) 1_555 . 1_555 N O5b P4 C2b 107.6(11) 1_555 . 1_555 N O6b P4 C2b 108.8(11) 1_555 . 1_555 N La O2b P3 131.3(15) 2_546 . 1_555 N La O5b P4 158.8(23) 2_646 . 1_555 N La O6b P4 156.2(25) 2_645 . 1_555 N P3 C1b N2 101.1(17) 1_555 . 1_555 N N1 C2b P4 131.8(26) 1_555 . 1_555 N C2 N2 C1b 107.8(14) 1_555 . 1_555 N C2 N2 C8 116.4(15) 1_555 . 1_555 N C1b N2 C8 117.4(15) 1_555 . 1_555 N N2 C8 C7 114.5(15) 1_555 . 1_555 N C8 C7 C6 117.1(16) 1_555 . 1_555 N C5 C6 C7 115.4(16) 1_555 . 1_555 N # Powder diffraction data for histogram 1 #============================================================================== # 9. INSTRUMENT CHARACTERIZATION _exptl_special_details ; ? ; # if regions of the data are excluded, the reason(s) are supplied here: _pd_proc_info_excluded_regions ; ? ; # The following item is used to identify the equipment used to record # the powder pattern when the diffractogram was measured at a laboratory # other than the authors' home institution, e.g. when neutron or synchrotron # radiation is used. _pd_instr_location ; ? ; _pd_calibration_special_details # description of the method used # to calibrate the instrument ; ? ; _diffrn_ambient_temperature 293 _diffrn_source ? _diffrn_source_target ? _diffrn_source_type ? _diffrn_measurement_device_type ? _diffrn_detector ? _diffrn_detector_type ? # make or model of detector _pd_meas_scan_method ? # options are 'step', 'cont', # 'tof', 'fixed' or # 'disp' (= dispersive) _pd_meas_special_details ; ? ; # The following two items identify the program(s) used (if appropriate). _computing_data_collection ? _computing_data_reduction ? # Describe any processing performed on the data, prior to refinement. # For example: a manual Lp correction or a precomputed absorption correction _pd_proc_info_data_reduction ? # The following item is used for angular dispersive measurements only. _diffrn_radiation_monochromator ? # The following items are used to define the size of the instrument. # Not all distances are appropriate for all instrument types. _pd_instr_dist_src/mono ? _pd_instr_dist_mono/spec ? _pd_instr_dist_src/spec ? _pd_instr_dist_spec/anal ? _pd_instr_dist_anal/detc ? _pd_instr_dist_spec/detc ? # 10. Specimen size and mounting information # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial ? # perpendicular to # equatorial plane _pd_spec_size_equat ? # parallel to # scattering vector # in transmission _pd_spec_size_thick ? # parallel to # scattering vector # in reflection _pd_spec_mounting # This field should be # used to give details of the # container. ; ? ; _pd_spec_mount_mode ? # options are 'reflection' # or 'transmission' _pd_spec_shape ? # options are 'cylinder' # 'flat_sheet' or 'irregular' loop_ _atom_type_symbol _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source La 2.0 -2.214 3.142 20.5780 2.94817 19.5990 0.24448 11.3727 18.7726 3.28719 133.124 2.14678 International_Tables_Vol_C P 8.0 0.001 0.016 6.43450 1.90670 4.17910 27.1570 1.78000 0.52600 1.49080 68.1645 1.11490 International_Tables_Vol_C O 28.0 -0.004 0.001 3.04850 13.2771 2.28680 5.70110 1.54630 0.32390 0.86700 32.9089 0.25080 International_Tables_Vol_C C 20.0 -0.002 0.000 2.31000 20.8439 1.02000 10.2075 1.58860 0.56870 0.86500 51.6512 0.21560 International_Tables_Vol_C N 4.0 -0.003 0.000 12.2126 0.00570 3.13220 9.89330 2.01250 28.9975 1.16630 0.58260 -11.529 International_Tables_Vol_C _diffrn_radiation_probe x-ray _diffrn_radiation_polarisn_ratio ? _diffrn_radiation_wavelength 1.5406 _diffrn_radiation_type ? _pd_proc_ls_prof_R_factor 0.0684 _pd_proc_ls_prof_wR_factor 0.0946 _pd_proc_ls_prof_wR_expected 0.0221 _refine_ls_R_Fsqd_factor 0.12184 _pd_proc_ls_background_function ; GSAS Background function number 1 with 20 terms. Shifted Chebyshev function of 1st kind 1: 1647.82 2: -1486.05 3: 880.627 4: -425.360 5: 181.121 6: -30.2813 7: -69.6481 8: 88.6265 9: -79.7150 10: 16.9672 11: 28.8771 12: -47.6654 13: 28.1020 14: 4.80831 15: -42.4080 16: 38.1946 17: -26.3533 18: 17.2604 19: -14.3381 20: 14.3706 ; _exptl_absorpt_process_details ; GSAS Absorption/surface roughness correction: function number 0 No correction is applied. ; _exptl_absorpt_correction_T_min 1.00000 _exptl_absorpt_correction_T_max 1.00000 _pd_proc_ls_profile_function ; CW Profile function number 4 with 21 terms Pseudovoigt profile coefficients as parameterized in P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. Asymmetry correction of L.W. Finger, D.E. Cox & A. P. Jephcoat (1994). J. Appl. Cryst.,27,892-900. Microstrain broadening by P.W. Stephens, (1999). J. Appl. Cryst.,32,281-289. #1(GU) = 0.000 #2(GV) = 0.000 #3(GW) = 4.193 #4(GP) = 0.000 #5(LX) = 2.148 #6(ptec) = 0.00 #7(trns) = 0.00 #8(shft) = 0.0000 #9(sfec) = 0.00 #10(S/L) = 0.0214 #11(H/L) = 0.0210 #12(eta) = 0.5327 #13(S400 ) = 1.4E-02 #14(S040 ) = 6.5E-03 #15(S004 ) = 1.7E+00 #16(S220 ) = 2.4E-02 #17(S202 ) = 3.5E-01 #18(S022 ) = -1.6E-02 #19(S301 ) = 1.2E-01 #20(S103 ) = 1.6E-01 #21(S121 ) = 2.5E-02 Peak tails are ignored where the intensity is below 0.0030 times the peak Aniso. broadening axis 0.0 0.0 1.0 ; _pd_proc_ls_peak_cutoff 0.00300 _pd_proc_info_datetime 2011-12-08T13:21:56 _pd_calc_method 'Rietveld Refinement' #---- raw/calc data loop ----- _pd_meas_2theta_range_min 4.0084 _pd_meas_2theta_range_max 99.9904 _pd_meas_2theta_range_inc 0.017 _pd_proc_2theta_range_min 3.9379 _pd_proc_2theta_range_max 99.9199 _pd_proc_2theta_range_inc 0.017 _reflns_number_total 1098 _reflns_limit_h_min 0 _reflns_limit_h_max 11 _reflns_limit_k_min 0 _reflns_limit_k_max 16 _reflns_limit_l_min -5 _reflns_limit_l_max 5 _reflns_d_resolution_high 1.091 _reflns_d_resolution_low 12.234 #--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--#